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Sodium Sulfate → 6-Methoxy-4-(4-{[5-oxo-1-(3-oxo-3,4-dihydro-2H-1,4-benzoxazin-6-yl)pyrrolidin-3-yl]amino}butyl)pyrido[2,3-b]pyrazin-3(4H)-one

HRID 1847040
ノート
印刷プレビュー

反応式

HRID 1847040 の反応式
[NH2:1][CH:2]1[CH2:6][N:5]([C:7]2[CH:8]=[CH:9][C:10]3[O:15][CH2:14][C:13](=[O:16])[NH:12][C:11]=3[CH:17]=2)[C:4](=[O:18])[CH2:3]1.[CH3:19][O:20][C:21]1[CH:22]=[CH:23][C:24]2[N:29]=[CH:28][C:27](=[O:30])[N:26]([CH2:31][CH2:32][CH2:33][CH:34]=O)[C:25]=2[N:36]=1.S([O-])([O-])(=O)=O.[Na+].[Na+].C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].C(=O)([O-])O.[Na+]>CN(C)C=O.ClCCl>[CH3:19][O:20][C:21]1[CH:22]=[CH:23][C:24]2[N:29]=[CH:28][C:27](=[O:30])[N:26]([CH2:31][CH2:32][CH2:33][CH2:34][NH:1][CH:2]3[CH2:3][C:4](=[O:18])[N:5]([C:7]4[CH:8]=[CH:9][C:10]5[O:15][CH2:14][C:13](=[O:16])[NH:12][C:11]=5[CH:17]=4)[CH2:6]3)[C:25]=2[N:36]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 24436Sodium SulfateHCID 516892Sodium BicarbonateHCID 5049666Sodium triacetoxyborohydrideHCID 824984066-(4-Amino-2-oxopyrrolidin-1-yl)-2H-1,4-benzoxazin-3(4H)-oneHCID 867249644-(6-Methoxy-3-oxopyrido[2,3-b]pyrazin-4(3H)-yl)butanal

生成物 1

HCID 60161643
6-Methoxy-4-(4-{[5-oxo-1-(3-oxo-3,4-dihydro-2H-1,4-benzoxazin-6-yl)pyrrolidin-3-yl]amino}butyl)pyrido[2,3-b]pyrazin-3(4H)-one
収率 18.5%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 6344Dichloromethane溶媒

実験手順

In N,N-dimethylformamide (5 ml) were dissolved 6-(4-Amino-2-oxopyrrolidin-1-yl)-2H-1,4-benzoxazin-3(4H)-one (Reference Example 6; 148 mg, 0.60 mmol) and 4-(6-methoxy-3-oxopyrido[2,3-b]pyrazin-4(3H)-yl)butanal (148 mg, 0.60 mmol). Sodium sulfate (1.0 g) was added to this solution and the mixture was stirred overnight at room temperature. Sodium triacetoxyborohydride (508 mg, 2.40 mmol) was added to the reaction solution and the mixture was stirred at room temperature for 6 hours. After completion of the reaction, the reaction solution was diluted with dichloromethane, basified by adding a saturated sodium hydrogen carbonate aqueous solution, and the organic layer was then separated and washed in the order of saturated sodium chloride solution, water (3×) and saturated sodium chloride solution. The organic layer was dried over anhydrous magnesium sulfate and the solvent was removed under reduced pressure. The obtained residue was purified by silica gel column chromatography (chloroform/methanol) to yield 53 mg (18%) of the title compound in the form of a light yellow foamy solid.

後処理

  1. stirringthe mixture was stirred at room temperature for 6 hours
  2. customAfter completion of the reaction
  3. customthe organic layer was then separated
  4. washwashed in the order of saturated sodium chloride solution, water (3×) and saturated sodium chloride solution
  5. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  6. customthe solvent was removed under reduced pressure
  7. customThe obtained residue was purified by silica gel column chromatography (chloroform/methanol)

出典と根拠

ORDレコード
ord-1955345b3da24db6987f4b72db334365
出典データセット
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08952010B2

反応ノート

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